US3783010A - Refracting,light permeable oxide layer and method for its manufacture - Google Patents
Refracting,light permeable oxide layer and method for its manufacture Download PDFInfo
- Publication number
- US3783010A US3783010A US00132041A US3783010DA US3783010A US 3783010 A US3783010 A US 3783010A US 00132041 A US00132041 A US 00132041A US 3783010D A US3783010D A US 3783010DA US 3783010 A US3783010 A US 3783010A
- Authority
- US
- United States
- Prior art keywords
- layer
- layers
- zirconium
- tantalum
- light permeable
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title description 17
- 238000004519 manufacturing process Methods 0.000 title description 11
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 abstract description 18
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052726 zirconium Inorganic materials 0.000 abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 239000010410 layer Substances 0.000 description 90
- 239000000203 mixture Substances 0.000 description 23
- 230000003287 optical effect Effects 0.000 description 14
- 229910052715 tantalum Inorganic materials 0.000 description 12
- 239000011521 glass Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 8
- 230000008016 vaporization Effects 0.000 description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 7
- 238000007740 vapor deposition Methods 0.000 description 7
- 238000010894 electron beam technology Methods 0.000 description 6
- 239000007858 starting material Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000001771 vacuum deposition Methods 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/245—Oxides by deposition from the vapour phase
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- G02B1/105—
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/23—Mixtures
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/151—Deposition methods from the vapour phase by vacuum evaporation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
- Y10T428/264—Up to 3 mils
- Y10T428/265—1 mil or less
Definitions
- a highly retracting, light permeable oxide layer on a support comprises oxygen, zirconium and tantalum, the ratio of the number of tantalum atoms to zirconium atoms being in the range of about 1:1 to 1:2.
- the invention relates to the production of optical layers by vacuum deposition.
- Oxidic protecting layers serve, for example, the purpose to protect sensitive surfaces of, for example, lenses, surface mirrors and the like objects against corrosion and mechanical injury or damage.
- Oxidic protecting layers serve, for example, the purpose to protect sensitive surfaces of, for example, lenses, surface mirrors and the like objects against corrosion and mechanical injury or damage.
- oxidic layers are commonly used as reflection reducing coatings, interference filters, beam or ray dividers, heat filters, cold light mirrors and coatings for spectacle lenses and the like.
- the mechanical and optical characteristics of such oxidic layers are dependent not only on the nature of the oxide which has been deposited on the respective surface, but also to a very pronounced extent on the manner in which the layer has been deposited.
- the starting substance or substances is or are admixed with one or several rare earth elements or compounds.
- zirconium oxide layers which, due to their high index of refraction and their nonabsorptiveness in the visible spectral region and their mechanical characteristics have been proposed for the construction of optical layer systems, unfortunately exhibit a very pronounced negative inhomogeneity. This strongly reduces, for example, the effectiveness of a reflection-reducing coating composed of such a layer.
- Various attempts have been made to eliminate this negative inhomogeneity by changing the deposition procedure, but all these attempts have failed.
- Some deposited layers exhibit a positive inhomogeneity.
- Another object of the invention is to provide a method for producing a layer of this kind which is exceedingly simple to carry out with a minimum of expenditure.
- the above objects are superiorly achieved by providing a layer on a support, which layer essentially consists of oxygen, zirconium and tantalum, the ratio of the number of tantalum atoms to zirconium atoms being in the range of 1:1 to 1:2.
- a mixture containing the elements zirconium and tantalum in metallic or oxidic form, at least one of the elements being present in oxidic form is heated under vacuum conditions to vaporize the mixture, whereupon the vapor is condensed on the support to be coated.
- Example 1 This test was carried out in a heatable vaporizing crucible of a vacuum deposition plant.
- a mixture consisting of 30% of metallic tantalum, calculated on the weight of the total mixture, and 70% of zirconium oxide (ZrO were inserted into the crucible.
- the crucible was heated with a wattage of about 2.5 kw. This resulted in a temperature of the mixture in the crucible of about 1800 C.
- a support in the form of a glass plate was arranged in the plant opposite the crucible, and the heating resulted in vaporiza tion of the material in the crucible and the deposition of a layer of a thickness of 250 nm. with a growing speed of 35 nm. per minute.
- the temperature of the glass plate was about 300 C.
- the vapor deposition was carried out in known manner in an oxygen atmosphere of mm. Hg. A layer was obtained which adhered satisfactorily to the glass plate, which was hard and completely absorptionfree in the visible spectral region.
- the constant index of refraction can be easily confirmed by proceeding in the following manner:
- a layer to be investigated is vapor-deposited on a glass plate with a low index of refraction until, upon illumination with light of a predetermined wave length, a minimum of the reflection occurs. If the deposited layer is homogeneous, then the reflection capability of the surface of the glass plate on which the layer has been deposited, should not differ from the respective wave length from the reflection capability of the uncoated glass surface. A layer is then present which conforms to the equation wherein A indicates the respective wave length, n is the index of refraction of the layer material and d is the thickness of the layer. By contrast, a higher reflection capability relative to the uncoated glass surface is obtained if the layer is positively inhomogeneous while a lower reflection capability as compared to that of the uncoated glass surface is obtained if the layer is negatively inhomogeneous.
- the deposition was carried out in a customary vacuum vapor deposition plant.
- the starting mixtures were in each case heatedin a crucible to a sufficient temperature, for example, 1700 to 1800 C., so as to result in vaporization of the starting mixture.
- the manner of heating the mixture in the crucible is not critical and can be efiected by known ways, for example, a tungsten crucible may be used which is heated by electric resistance heating, or the heating is effected by means of an electron beam. In the latter case, the electron beam is directed onto the surface of the mixture to be vaporized which thus is directly heated to the evaporation temperature.
- the heat efiect of the electron beam is, as is known, the product of the current intensity of the beam and the applied potential.
- layers were obtained which are completely homogeneous in the above indicated sense, although the deposition was carried out with a growth rate of the layers on the support of about 350 A per minute up to layer thicknesses of about 300 nm.
- the layers obtained in accordance with the invention may be used for numerous purposes. For example, they are extremely suitable, as already mentioned, for the build-up of multi-layer coatings. Such multi-layer coatings, as compared to single-layer reflection-reducing coatings have the advantage that they result in a significantly stronger reduction of the reflection of a coated surface.
- the tantalum-suboxide mentioned in Table 2 may be obtained by melting together a stoichiometric mixture of tantalum metal and tantalum-pentoxide while the mentioned zirconium-suboxide may be obtained by melting together a stoichiometric mixture of zirconium metal and zirconium-dioxide.
- the melting-together may be effected in advance of the vapor deposition in a preceding step to obtain the respective suboxide, or it may be effected in the vaporizing crucible proper in which event the starting mixture contains three components.
- the crucible would be fed with a mixture of metallic tantalum, Ta O and ZrO while, in respect to Example 7, the mixture in the crucible would consist of Ta O Zr and ZrO
- the inventive procedure results in the formation of layers of predetermined composition, to wit, the layer consists of oxygen, tantalum and zirconium. It is assumed that in the ideal case, the ratio of the number of atoms of tantalum to the number of atoms of zirconium is about 1:1.5. For practical requirements, however, it is not necessary to adhere to this theoretical value, but values deviating therefrom also give excellent results.
- the measurement of the ratio is subject to measuring errors.
- the atomic ratio in the inventive layer is always within a limit range and that the ratio of the number of tantalum atoms to the number of zirconium atoms is thus always between 1:1 to 1:2.
- investigations by X-ray diagrams have indicated that the inventive layers do not contain any crystalline zirconium oxide, or if crystalline zirconium oxide is contained in them, the amount is extremely small. This explains the superior homogeneity of the inventive layers.
- inventive layers may be successfully employed for interference systems with satisfactory ultraviolet permeability. This is so because the layers up to a value of about 340 nm. may be produced without exhibiting any absorption whatsoever.
- the single figure shows a support having an inventive layer deposited thereon.
- the support in the form of a glass plate, has deposited thereon the layer 2 consisting of tantalum, zirconium and oxygen.
- the layer is light permeable and highly retracting, and essentially consists of oxygen, zirconium and tantalum, the ratio of the number of tantalum atoms to zirconium atoms in the layer being in the range of 1:136 to 1:1.7, said layer being essentially devoid of crystalline zirconium oxide.
Landscapes
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Optics & Photonics (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Physical Vapour Deposition (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Surface Treatment Of Glass (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH549170A CH527916A (de) | 1970-04-13 | 1970-04-13 | Verfahren zur Herstellung einer hochbrechenden lichtdurchlässigen Oxidschicht |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3783010A true US3783010A (en) | 1974-01-01 |
Family
ID=4294470
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00132041A Expired - Lifetime US3783010A (en) | 1970-04-13 | 1971-04-07 | Refracting,light permeable oxide layer and method for its manufacture |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US3783010A (de) |
| JP (1) | JPS5430997B1 (de) |
| AT (1) | AT305515B (de) |
| CH (1) | CH527916A (de) |
| DE (1) | DE2050556C3 (de) |
| FR (1) | FR2086008B1 (de) |
| GB (1) | GB1328298A (de) |
| NL (1) | NL142459B (de) |
| SE (1) | SE358143B (de) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3900609A (en) * | 1970-04-13 | 1975-08-19 | Balzers Patent Beteilig Ag | Method for manufacture of a refracting, light permeable oxide layer |
| US4260222A (en) * | 1978-07-11 | 1981-04-07 | Olympus Optical Co., Ltd. | Multi-layer non-reflecting film |
| WO2004067463A1 (en) * | 2003-01-28 | 2004-08-12 | Philips Intellectual Property & Standards Gmbh | Transparent zirconium oxide - tantalum and/or tantalum oxide coating |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3009533C2 (de) * | 1980-03-12 | 1986-11-06 | D. Swarovski & Co., Wattens, Tirol | Belag mit mittlerem Brechwert, Verfahren zu dessen Herstellung und Verwendung des Belages |
| DE3026703C2 (de) * | 1980-07-15 | 1983-01-27 | Will Wetzlar Gmbh, 6330 Wetzlar | Verfahren zur Herstellung eines Antireflexbelages auf einem transparenten Material, wie einem optischen Glas |
| JPS5931147A (ja) * | 1982-08-17 | 1984-02-20 | 株式会社豊田中央研究所 | 可視光透過性熱線しやへい膜およびその製造方法 |
| JP6645012B2 (ja) * | 2015-01-29 | 2020-02-12 | 日亜化学工業株式会社 | 蒸着材料 |
-
1970
- 1970-04-13 CH CH549170A patent/CH527916A/de not_active IP Right Cessation
- 1970-06-12 NL NL707008641A patent/NL142459B/xx not_active IP Right Cessation
- 1970-10-15 DE DE2050556A patent/DE2050556C3/de not_active Expired
-
1971
- 1971-03-24 AT AT255071A patent/AT305515B/de not_active IP Right Cessation
- 1971-03-30 FR FR7111148A patent/FR2086008B1/fr not_active Expired
- 1971-04-07 SE SE04591/71A patent/SE358143B/xx unknown
- 1971-04-07 US US00132041A patent/US3783010A/en not_active Expired - Lifetime
- 1971-04-13 JP JP2284671A patent/JPS5430997B1/ja active Pending
- 1971-04-19 GB GB2614571*A patent/GB1328298A/en not_active Expired
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3900609A (en) * | 1970-04-13 | 1975-08-19 | Balzers Patent Beteilig Ag | Method for manufacture of a refracting, light permeable oxide layer |
| US4260222A (en) * | 1978-07-11 | 1981-04-07 | Olympus Optical Co., Ltd. | Multi-layer non-reflecting film |
| WO2004067463A1 (en) * | 2003-01-28 | 2004-08-12 | Philips Intellectual Property & Standards Gmbh | Transparent zirconium oxide - tantalum and/or tantalum oxide coating |
| US20060280950A1 (en) * | 2003-01-28 | 2006-12-14 | Arnd Ritz | Transparent zirconium oxide-tantalum and/or tantalum oxide coating |
| US7521871B2 (en) | 2003-01-28 | 2009-04-21 | Koninklijke Philips Electronics, N.V. | Transparent zirconium oxide-tantalum and/or tantalum oxide coating |
Also Published As
| Publication number | Publication date |
|---|---|
| NL7008641A (de) | 1971-10-15 |
| NL142459B (nl) | 1974-06-17 |
| CH527916A (de) | 1972-09-15 |
| GB1328298A (en) | 1973-08-30 |
| AT305515B (de) | 1973-02-26 |
| DE2050556B2 (de) | 1973-06-20 |
| DE2050556C3 (de) | 1978-11-30 |
| JPS5430997B1 (de) | 1979-10-04 |
| SE358143B (de) | 1973-07-23 |
| FR2086008A1 (de) | 1971-12-31 |
| DE2050556A1 (de) | 1971-12-02 |
| FR2086008B1 (de) | 1975-06-06 |
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